CN108807870A - A kind of preparation method of lithium-ion negative pole high power capacity composite material - Google Patents
A kind of preparation method of lithium-ion negative pole high power capacity composite material Download PDFInfo
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- CN108807870A CN108807870A CN201810379358.8A CN201810379358A CN108807870A CN 108807870 A CN108807870 A CN 108807870A CN 201810379358 A CN201810379358 A CN 201810379358A CN 108807870 A CN108807870 A CN 108807870A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention discloses a kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, is then added in 10 times of the ethanol solution that quality is the sub- silicon of oxidation；2）The asphalt powder that the quality of the sub- silicon of oxidation is 2%-15% is added in the solution mixed, then slurry is put into high energy ball mill and carries out ball milling；3）After grinding, spraying treatment is dried to slurry；4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature carbon coating processing.The present invention carries out compound SiO materials using carbon material, then metallic aluminium powder is added in the composite to be doped, modified SiO composite materials as cathode click it, and coulombic efficiency can reach 80% or more for the first time, after repeatedly recycling, the specific discharge capacity of composite material remains to be maintained at 850mAh/g or more, meets the needs used.
Description
Technical field
The present invention relates to negative material field technologies, refer in particular to a kind of preparation of lithium-ion negative pole high power capacity composite material
Method.
Background technology
In recent years, the environmental problem manifested with traditional energy gradually becomes severe, various electronic products are increasingly
Universal and electric vehicle fast development, developing novel green high-capacity electrochmical power source becomes particularly urgent.Green energy resource
Optimum utilization, it is support to need the energy storage of long-life, high-energy-density and specific power and electrical source of power.Lithium ion battery has work
Voltage is high, it is bigger than energy, have extended cycle life, self-discharge rate is low, memory-less effect and it is environmentally friendly the advantages that, be a new generation
The important development direction of the energy.Currently, the application of lithium rechargeable battery commercially negative material is mainly Carbon materials.So
And carbon material there are theoretical capacities relatively low, during overcharge safety it is poor the problems such as, make it be difficult to meet high capacity power source
It is required that.Find the key point that novel anode material with high performance is lithium ion battery future development.
Silicon is high with its theoretical capacity, resourceful and have many advantages, such as discharge potential close to lithium or graphite, is considered
It is the negative material being expected to instead of carbon.But silicon as negative material there are an extremely serious problem, silicium cathode is after discharge
There is extremely serious bulk effect, greatly expansion is so that avalanche occurs for the structure of material, and then influences following for electrode material
Ring performance.And SiO has the specific capacity (2443mAh/g) higher than business carbon material and preferably excellent cycle performance, it can
Lithium is largely absorbed and stored, is carbon negative electrode material of lithium ion cell very one of the direction with development potentiality.However the sub- silicon of oxidation
The shortcomings of material by research finds it, and that there are first charge-discharge efficiencies is relatively low, and electric conductivity is poor.
Chinese invention patent application publication No. CN 104425806A disclose a kind of lithium cell cathode material and its preparation side
Method, method are：
（1）Aluminium powder is mixed with the sub- silicon of oxidation, wherein the grain size of aluminium powder is 10m, and the grain size for aoxidizing sub- silicon is 30m, and is put into row
In celestial body grinding machine under 300rmp rotating speeds ball milling 8h, obtain mixture, which includes the sub- silicon of oxidation and aluminium powder, wherein
The mass ratio of the sub- silicon of oxidation and aluminium powder is 1.7:1.When the sub- silicon of the oxidation and the mass ratio of the aluminium are 1.7：When 1, aluminium plays
The abundant purpose for reducing the active oxygen in final ion cathode material lithium obtained, improves the charge and discharge of ion cathode material lithium
First charge discharge efficiency.
（2）By step（1）In obtained mixture be put into the high temperature furnace of vacuum condition, with the heating speed of 4 DEG C/min
Degree is warming up to 1000 DEG C, and calcination 10 hours obtains lithium ion battery negative material.
In the above-mentioned methods, material after multiple charge and discharge, reversible capacity 700mAh/g, reversible capacity is smaller,
It cannot meet the needs.
Invention content
In view of this, in view of the deficiencies of the prior art, the present invention aims to provide a kind of lithium-ion negative poles
The preparation method of high power capacity composite material can effectively solve the problems, such as that existing negative material reversible capacity is small.
To achieve the above object, the present invention is using following technical solution：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in；
2）The asphalt powder that the quality of the sub- silicon of oxidation is 2%-15% is added in the solution mixed, slurry is then put into high energy
Ball milling is carried out in ball mill；
3）After grinding, spraying treatment is dried to slurry；
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out pyrocarbon packet
Cover processing；
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
As a preferred embodiment, the step 2）It is middle asphalt powder is put into mixed solution after, stir 8-12min, so
The solution mixed is put into high energy ball mill again afterwards and is ground, time 2-4h, rotating speed 500-700r/m.
As a preferred embodiment, the step 3）Its feeding temperature of middle spray drying treatment is 250-350 DEG C, outlet temperature
Degree is 90-100 DEG C.
As a preferred embodiment, the step 4）Middle heating is under atmosphere of inert gases, and tube furnace is with 3-7 DEG C/min
Speed heating, 2-4h is kept the temperature after being heated to 800-1000 DEG C, then natural cooling.
The present invention has clear advantage and advantageous effect compared with prior art, specifically, by above-mentioned technical proposal
Known to：
The present invention carries out compound SiO materials using carbon material, and metallic aluminium powder is then added in the composite and is doped, changes
SiO composite materials after property as cathode click it, and coulombic efficiency can reach 80% or more for the first time, after repeatedly recycling,
The specific discharge capacity of composite material remains to be maintained at 850mAh/g or more, meets the needs used.
Description of the drawings
Fig. 1 is the SEM figures for the lithium battery composite material that the present invention obtains；
Fig. 2 is the curve graph of specific discharge capacity of the present invention and cycle-index.
Specific implementation mode
Present invention is disclosed a kind of preparation methods of lithium-ion negative pole high power capacity composite material, include following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 2%-15% is added in the solution mixed, is then put into slurry
Ball milling is carried out in high energy ball mill.After asphalt powder is put into mixed solution, 8-12min is stirred, it is then molten by what is mixed again
Liquid is put into high energy ball mill and is ground, time 2-4h, rotating speed 500-700r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 250-350
DEG C, outlet temperature is 90-100 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 3-7 DEG C/min, is heated to 800-1000
2-4h is kept the temperature after DEG C, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
The present invention is described in further details with multiple embodiments below：
Embodiment 1：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 10% is added in the solution mixed, slurry is then put into height
Ball milling can be carried out in ball mill.After asphalt powder is put into mixed solution, 10min is stirred, then again puts the solution mixed
Enter in high energy ball mill and is ground, time 3h, rotating speed 600r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 300 DEG C, is gone out
Mouth temperature is 95 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 5 DEG C/min, is kept the temperature after being heated to 900 DEG C
3h, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
SEM if Fig. 1 is the lithium battery composite material obtained in the present embodiment schemes, it can be seen from figure 1 that after asphalt high-temperature cracking
SiO and Al is coated glomeration by the carbon of formation.
After button battery is made in SiO composite materials, by Land cell testers test battery at different conditions
Charge-discharge performance, as shown in Fig. 2, being the curve graph of specific discharge capacity and cycle-index in the present embodiment, by repeatedly recycling survey
After examination, its reversible specific capacity of material made from the present embodiment remains to be maintained at 1000mAh/g or so, and coulombic efficiency reaches for the first time
88%。
Embodiment 2：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 2% is added in the solution mixed, slurry is then put into high energy
Ball milling is carried out in ball mill.After asphalt powder is put into mixed solution, 8min is stirred, the solution mixed is then put into height again
It can be ground in ball mill, time 2h, rotating speed 500r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 250 DEG C, is gone out
Mouth temperature is 90 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 4 DEG C/min, is kept the temperature after being heated to 800 DEG C
2h, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
After multiple loop test, its reversible specific capacity of material made from the present embodiment remains to be maintained at the left sides 990mAh/g
The right side, for the first time coulombic efficiency reach 85%.
Embodiment 3：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 15% is added in the solution mixed, slurry is then put into height
Ball milling can be carried out in ball mill.After asphalt powder is put into mixed solution, 11min is stirred, then again puts the solution mixed
Enter in high energy ball mill and is ground, time 4h, rotating speed 550r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 280 DEG C, is gone out
Mouth temperature is 100 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 3 DEG C/min, is protected after being heated to 1000 DEG C
Warm 4h, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
After multiple loop test, its reversible specific capacity of material made from the present embodiment remains to be maintained at the left sides 980mAh/g
The right side, for the first time coulombic efficiency reach 82%.
Embodiment 4：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 12% is added in the solution mixed, slurry is then put into height
Ball milling can be carried out in ball mill.After asphalt powder is put into mixed solution, 9min is stirred, is then again put into the solution mixed
It is ground in high energy ball mill, time 3h, rotating speed 650r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 300 DEG C, is gone out
Mouth temperature is 94 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 7 DEG C/min, is kept the temperature after being heated to 850 DEG C
2.5h, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
After multiple loop test, its reversible specific capacity of material made from the present embodiment remains to be maintained at the left sides 900mAh/g
The right side, for the first time coulombic efficiency reach 81%.
Embodiment 5：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 13% is added in the solution mixed, slurry is then put into height
Ball milling can be carried out in ball mill.After asphalt powder is put into mixed solution, 12min is stirred, then again puts the solution mixed
Enter in high energy ball mill and is ground, time 2h, rotating speed 700r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 350 DEG C, is gone out
Mouth temperature is 93 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 6 DEG C/min, is kept the temperature after being heated to 950 DEG C
3.5h, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
After multiple loop test, its reversible specific capacity of material made from the present embodiment remains to be maintained at the left sides 900mAh/g
The right side, for the first time coulombic efficiency reach 81%.
Embodiment 6：
A kind of preparation method of lithium-ion negative pole high power capacity composite material, includes following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in.
2）The asphalt powder that the quality of the sub- silicon of oxidation is 8% is added in the solution mixed, slurry is then put into high energy
Ball milling is carried out in ball mill.After asphalt powder is put into mixed solution, 10min is stirred, is then again put into the solution mixed
It is ground in high energy ball mill, time 4h, rotating speed 680r/m.
3）After grinding, spraying treatment is dried to slurry.Its feeding temperature of spray drying treatment is 320 DEG C, is gone out
Mouth temperature is 98 DEG C.
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out high temperature
Carbon coating processing.Heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 3 DEG C/min, is kept the temperature after being heated to 880 DEG C
3h, then natural cooling.
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
After multiple loop test, its reversible specific capacity of material made from the present embodiment remains to be maintained at the left sides 850mAh/g
The right side, for the first time coulombic efficiency reach 80%.
The design focal point of the present invention is：The present invention carries out compound SiO materials using carbon material, then in composite material
Middle addition metallic aluminium powder is doped, and modified SiO composite materials as cathode click it, and coulombic efficiency can reach for the first time
80% or more, after repeatedly recycling, the specific discharge capacity of composite material remains to be maintained at 850mAh/g or more, meets and uses
Needs.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore it is every according to the technical essence of the invention to any subtle modifications, equivalent variations and modifications made by above example, still
Belong in the range of technical solution of the present invention.
Claims (4)
1. a kind of preparation method of lithium-ion negative pole high power capacity composite material, it is characterised in that：Include following steps：
1）A certain amount of SiO powder is weighed, according to 2:1 ratio is mixed with aluminium powder, and it is the sub- silicon of oxidation to be then added to quality
10 times of ethanol solution in；
2）The asphalt powder that the quality of the sub- silicon of oxidation is 2%-15% is added in the solution mixed, slurry is then put into high energy
Ball milling is carried out in ball mill；
3）After grinding, spraying treatment is dried to slurry；
4）The composite powder crossed by dry spraying treatment is collected, is placed into tube furnace and is heated to carry out pyrocarbon packet
Cover processing；
5）It is beaten after cooling, is prepared into electrode, carry out correlated performance detection.
2. a kind of preparation method of lithium-ion negative pole high power capacity composite material according to claim 1, it is characterised in that：Institute
State step 2）It is middle asphalt powder is put into mixed solution after, stir 8-12min, the solution mixed is then put into high energy ball again
It is ground in grinding machine, time 2-4h, rotating speed 500-700r/m.
3. a kind of preparation method of lithium-ion negative pole high power capacity composite material according to claim 1, it is characterised in that：Institute
State step 3）Its feeding temperature of middle spray drying treatment is 250-350 DEG C, and outlet temperature is 90-100 DEG C.
4. a kind of preparation method of lithium-ion negative pole high power capacity composite material according to claim 1, it is characterised in that：Institute
State step 4）Middle heating is under atmosphere of inert gases, and tube furnace is heated up with the speed of 3-7 DEG C/min, is heated to 800-1000 DEG C
After keep the temperature 2-4h, then natural cooling.
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| CN110550635A (en) * | 2019-09-15 | 2019-12-10 | 孔晓蕾 | Preparation method of novel carbon-coated silica negative electrode material |
| CN111438364A (en) * | 2020-04-07 | 2020-07-24 | 广东凯金新能源科技股份有限公司 | High-first-efficiency silicon-based composite material and preparation method thereof |
| CN112652744A (en) * | 2019-10-12 | 2021-04-13 | 江苏天奈科技股份有限公司 | Preparation method of high-capacity high-cycle lithium battery negative electrode material and lithium battery |
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Application publication date: 20181113 |